CN103713063B - Method for simultaneously and rapidly detecting contents of multiple heavy metal elements in salt - Google Patents
Method for simultaneously and rapidly detecting contents of multiple heavy metal elements in salt Download PDFInfo
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- CN103713063B CN103713063B CN201310754289.1A CN201310754289A CN103713063B CN 103713063 B CN103713063 B CN 103713063B CN 201310754289 A CN201310754289 A CN 201310754289A CN 103713063 B CN103713063 B CN 103713063B
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Abstract
The invention discloses a method for simultaneously and rapidly detecting the contents of multiple heavy metal elements in salt. The method comprises the following steps: pouring a salt solution into a 732 type cation exchange resin column at a certain flow velocity, exchanging hydrogen ions on a sulfonic acid group of resin in the resin column with sodions and heavy metal ions in the salt, and enriching the sodions and heavy metal ions in a salt solution; eluting the sodions adsorbed on the 732 type cation exchange resin column by using a diluent hydrochloric acid solution, removing the sodions, eluting the heavy metal ions on special resin by using a concentrated hydrochloric acid solution, and collecting a receiving solution in the step; and finally, measuring the collected receiving solution by using an inductively coupled plasma emission spectrometer, and measuring the contents of various heavy metal elements in the receiving solution. According to the method, a salt effect of the salt is overcome, the content of multiple heavy metals in the salt can be simultaneously, accurately and rapidly detected, and the method has the advantages of simplicity in operation, high analysis speed, high accuracy, high sensitivity and the like.
Description
Technical field
The method that the present invention relates to detection device for multi metallic elements content in a kind of while fast detecting salt, belongs to food safety detection field.
Technical background
As everyone knows, heavy metal element is quite large to the harm of human body, once heavy metal element enters human body, be accumulated to a certain degree, will with human body in important substance generation coordination, changed the normal physiological function of this material, even enter nervous system, the normal function of interference body and cause pathology, can cause death when serious.Salt is one of the mankind's most important material of depending on for existence, is also the most frequently used flavoring in culinary art.The mankind must absorb a certain amount of salt every day, the normal operation of guarantee body.Therefore, most important to the control of the contents of heavy metal elements in salt.
In salt, contents of heavy metal elements is an important indicator weighing salt quality and safety.Heavy metal element kind in salt is many, as copper, zinc, lead, cadmium and barium etc., still, due to the Specific salt effect of salt, can disturb the test generation of spectral class instrument, thereby being produced, result departs from more greatly, so that the content of the detection device for multi metallic elements in while Measurement accuracy salt of having no idea.At present, the domestic coherent detection standard of simultaneously measuring detection device for multi metallic elements content in salt that there is no, therefore, how to overcome salt effect, provide a kind of while accurately, the method for the content of detection device for multi metallic elements is the major issue facing in salt quality and safety detection in fast detecting salt.
Summary of the invention
The problem existing for overcoming prior art, the invention provides the method for detection device for multi metallic elements in a kind of while fast detecting salt, the method has overcome the salt effect of salt, can detect the content of detection device for multi metallic elements in salt simultaneously, and there is simple to operate, the advantage such as analysis speed is fast, accuracy is high and sensitivity is high.
Realizing the technical scheme that the object of the invention takes is:
In while fast detecting salt, a method for detection device for multi metallic elements, comprises the steps:
1) salt is added to the water, is mixed with the salt solution that concentration is 0.005g/mL～0.015g/mL;
2) salt solution is poured in 732 type cation exchange resin columns with the flow velocity of 3.0mL/min～4.0mL/min, the sodion in salt solution and heavy metal ion are carried out to enrichment;
3) hydrochloric acid solution that is 0.075mol/L～0.125mol/L by enough concentration carries out wash-out with the flow velocity of 3.5mL/min～5.5mL/min to 732 type cation exchange resin columns, removes the sodion being adsorbed on 732 type Zeo-karbs;
4) hydrochloric acid solution that is 2.5mol/L～3.5mol/L by concentration carries out wash-out with the flow velocity of 5.0mL/min～7.0mL/min to 732 type cation exchange resin columns, the heavy metal ion being adsorbed on 732 type Zeo-karbs is eluted, volume ratio >=1 ﹕ 5 of hydrochloric acid solution and salt solution, the solution that flows out this resin column after collection wash-out, is receiving liquid;
5) receiving liquid of collection is measured with inductive coupling plasma emission spectrograph, the each Heavy Metallic Elements in receiving liquid is carried out quantitatively and qualitative analysis.
When the volume of described salt solution is 500mL, when the diameter of 732 type cation exchange resin columns is 10mm～15mm, the height of controlling resin bed is 10cm～30cm.
Described each Heavy Metallic Elements comprises copper, zinc, cadmium, lead and barium.
Compared with prior art, advantage of the present invention and beneficial effect are:
First the method is poured salt solution in 732 type cation exchange resin columns, sodion and heavy metal ion in hydrogen ion and salt solution in this resin column on the sulfonic group of resin exchange, sodion in salt solution and heavy metal ion are carried out to enrichment, then wash away with rarer hydrochloric acid solution the sodion being adsorbed on 732 type Zeo-karbs, remove sodion, again with denseer hydrochloric acid solution wash away flow out after being adsorbed on the heavy metal ion on 732 type Zeo-karbs and collecting wash-out resin column receiving liquid, finally the receiving liquid of collection is measured with inductive coupling plasma emission spectrograph, each Heavy Metallic Elements in receiving liquid is carried out quantitatively and qualitative analysis.From the above, the method utilizes 732 type Zeo-karbs same to the adsorptive power of sodion and heavy metal ion in the hydrochloric acid solution of variable concentrations, hydrogen ion in the hydrochloric acid of variable concentrations successively carries out ion-exchange with sodion and the heavy metal ion of resin adsorption, before measuring the content of contents of many kinds of heavy metal ion with inductive coupling plasma emission spectrograph, remove sodion, thereby eliminate the salt effect of sodion to the spectrometric interference of heavy metal ion, and inductive coupling plasma emission spectrograph can carry out quantitatively and qualitative analysis various heavy simultaneously fast.
Therefore, the method has overcome the salt effect of salt, has eliminated sodion to the spectrometric interference of heavy metal ion, can carry out quantitative and qualitative analysis to detection device for multi metallic elements in salt simultaneously, and simple to operate, analysis speed is fast, accuracy and highly sensitive.
Embodiment
Below in conjunction with embodiment to the present invention to further detailed description.
For checking feasibility and the superiority of the method for detection device for multi metallic elements content in while fast detecting salt provided by the invention, in the time of preparation salt solution, add heavy metal mixed standard solution, adopt the method for detection device for multi metallic elements content in while fast detecting salt provided by the invention to detect the salt solution that contains heavy metal mixed standard solution, according to the difference of the concentration of the result concentration detecting and known heavy metal, feasibility and superiority to the method are assessed.
Embodiment 1
1) take 5g salt, add heavy metal mixed standard solution 1mL(Cu=10 μ g/mL, Zn=10 μ g/mL, Cd=1 μ g/mL, Pb=10 μ g/mL, Ba=10 μ g/mL) water dissolving, be settled in the volumetric flask of 500mL, be mixed with the salt solution that concentration is 0.01g/mL, the mark-on level that is each heavy metal ion in salt is Cu=2mg/kg, Zn=2mg/kg, Cd=0.2mg/kg, Pb=2mg/kg, Ba=2mg/kg;
2) salt solution of 500mL is poured in 732 type cation exchange resin columns with the flow velocity of 3.5mL/min, sodion and heavy metal ion are carried out to enrichment, the diameter in 732 type cation exchange resin columns is 10mm, and the height of controlling resin bed is 10cm;
3) with the flow velocity of 4.5mL/min, 732 type cation exchange resin columns are carried out to wash-out with the hydrochloric acid solution of 500mL0.1mol/L, remove the sodion being adsorbed on 732 type Zeo-karbs;
4) with the flow velocity of 6.0mL/min, 732 type cation exchange resin columns are carried out to wash-out with the hydrochloric acid solution of 100mL3mol/L, the heavy metal ion being adsorbed on 732 type Zeo-karbs is eluted, after collection wash-out, flow out the receiving liquid of resin column, in this step, hydrochloric acid solution and salt solution volume ratio can not be less than 1 ﹕ 5, heavy metal ion can not elute completely very little, but also not all right too much, there are two bad aspects, the one, waste, the 2nd, the content of heavy metal ion is original just seldom, add the amount of hydrochloric acid solution how no doubt can well heavy metal ion be eluted, also heavy metal ion is further diluted simultaneously, be diluted to the detectability that too low concentration may exceed inductive coupling plasma emission spectrograph, cause inductive coupling plasma emission spectrograph to detect not out, therefore, volume ratio is herein not there is no the upper limit, the volume of hydrochloric acid solution can not be excessive, the concentration that can not be diluted to heavy metal ion is too low, lower than the detection limit of inductive coupling plasma emission spectrograph,
5) receiving liquid of collection is measured with inductive coupling plasma emission spectrograph, the copper in receiving liquid, zinc, cadmium, lead and barium heavy metal element are carried out quantitatively and qualitative analysis.
6) in salt, the measurement result of contents of heavy metal elements is: Cu=1.68mg/kg, Zn=1.70mg/kg, Cd=0.160mg/kg, Pb=2.12mg/kg, Ba=2.18mg/kg; The recovery is respectively Cu:84%, Zn:85%, Cd:80%, Pb:106%, Ba:109%.
Embodiment 2
1) take 7.5g salt, add heavy metal mixed standard solution 15mL(Cu=10 μ g/mL, Zn=10 μ g/mL, Cd=1 μ g/mL, Pb=10 μ g/mL, Ba=10 μ g/mL) water dissolving, be settled in the volumetric flask of 500mL, be mixed with the salt solution that concentration is 0.015g/mL, the mark-on level that is each heavy metal ion content in salt is Cu=20mg/kg, Zn=20mg/kg, Cd=2mg/kg, Pb=20mg/kg, Ba=20mg/kg;
2) salt solution of 500mL is poured in 732 type cation exchange resin columns with the flow velocity of 4mL/min, sodion and heavy metal ion are carried out to enrichment, the diameter of 732 type cation exchange resin columns is 15mm, and the height of controlling resin bed is 30cm;
3) with the flow velocity of 5.5mL/min, 732 type cation exchange resin columns are carried out to wash-out with the hydrochloric acid solution of 500mL0.125mol/L, remove the sodion being adsorbed on 732 type Zeo-karbs;
4) with the flow velocity of 5.0mL/min, 732 type cation exchange resin columns are carried out to wash-out with the hydrochloric acid solution of 200mL2.5mol/L, the heavy metal ion being adsorbed on 732 type Zeo-karbs is eluted, after collection wash-out, flow out the receiving liquid of resin column;
5) receiving liquid of collection is measured with inductive coupling plasma emission spectrograph, the copper in receiving liquid, zinc, cadmium, lead and barium heavy metal element are carried out quantitatively and qualitative analysis.
6) in salt, the measurement result of contents of heavy metal elements is: Cu=18.8mg/kg, Zn=19.2mg/kg, Cd=1.78mg/kg, Pb=20.4mg/kg, Ba=20.8mg/kg; The recovery is respectively Cu:94%, Zn:96%, Cd:89%, Pb:102%, Ba:104%.
The result detecting according to embodiment 1 and embodiment 2 can be found out, the recovery of Cu, Zn, Cd, Pb and Ba element is substantially all more than 80%, especially the recovery of Pb and Ba element is all higher than 100%, the method that detection device for multi metallic elements content in while fast detecting salt provided by the invention is described is the content of Cu, Zn, Cd, Pb and Ba element in fast detecting salt simultaneously, and sensitivity and accuracy high, especially Pb and Ba element, sensitivity and accuracy are quite high.
Show thus the content of detection device for multi metallic elements in the method for detection device for multi metallic elements content energy while fast detecting salt in while fast detecting salt provided by the invention, and accuracy and highly sensitive.
Claims (3)
1. a method for detection device for multi metallic elements content in while fast detecting salt, is characterized in that comprising the steps:
1) salt is added to the water, is mixed with the salt solution that concentration is 0.005g/mL～0.015g/mL;
2) salt solution is poured in 732 type cation exchange resin columns with the flow velocity of 3.0mL/min～4.0mL/min, the sodion in salt solution and heavy metal ion are carried out to enrichment;
3) hydrochloric acid solution that is 0.075mol/L～0.125mol/L by enough concentration carries out wash-out with the flow velocity of 3.5mL/min～5.5mL/min to 732 type cation exchange resin columns, removes the sodion being adsorbed on 732 type Zeo-karbs;
4) hydrochloric acid solution that is 2.5mol/L～3.5mol/L by concentration carries out wash-out with the flow velocity of 5.0mL/min～7.0mL/min to 732 type cation exchange resin columns, the heavy metal ion being adsorbed on 732 type Zeo-karbs is eluted, volume ratio >=1 ﹕ 5 of hydrochloric acid solution and salt solution, the solution that flows out this resin column after collection wash-out, is receiving liquid;
5) receiving liquid of collection is measured with inductive coupling plasma emission spectrograph, the each Heavy Metallic Elements in receiving liquid is carried out quantitatively and qualitative analysis.
2. the method for detection device for multi metallic elements content in fast detecting salt simultaneously according to claim 1, it is characterized in that: when the volume of described salt solution is 500mL, when the diameter of 732 type cation exchange resin columns is 10mm～15mm, the height of controlling resin bed is 10cm～30cm.
3. the method for detection device for multi metallic elements content in fast detecting salt simultaneously according to claim 1, is characterized in that: described each Heavy Metallic Elements comprises copper, zinc, cadmium, lead and barium.
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| CN106053359A (en) * | 2016-05-18 | 2016-10-26 | 中华人民共和国淮安出入境检验检疫局 | Method using static adsorption ion exchange technology to separate and measure copper ions in salt |
| CN112044478A (en) * | 2020-09-02 | 2020-12-08 | 广东力恩普健康产业科技有限公司 | Method for removing harmful metal ions in pineapple peel juice |
| CN113754122B (en) * | 2021-09-18 | 2022-11-25 | 南京昆腾化工科技有限公司 | Process for removing sodium by returning electroplating heavy metal ions to tank |
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